The primary objective of this project is to evaluate the capabilities of various micro-separation techniques (capillary electrophoresis, capillary electrochromatography, capillary HPLC as well as hybrid methods) for the analysis of biologically and pharmaceutically important samples. A protocol will be developed that allows testing of a broad range of solute classes from small molecules thoroughly macromolecules in order to determine the most suitable method(s) for solving a particular type of separation problem. Because samples related to biological, physiological or pharmaceutical processes are often limited in size or amount of material, the use of micro-separation techniques is highly desirable. The protocol described in this proposal should provide both a better fundamental understanding of micro-separation methods and their interrelationships as well as a practical guide to other scientists for selecting the most appropriate means for various types of biomolecule and pharmaceutical analyses.